Method of and apparatus for separating petroleum sludge



sept. 7, 1926.- 1,599,360

l. HECHENBLEIKNER ET AL METHOD 0F AND APPARATUS FOR SEPARATING PETROLEUM SLUDGE Filed March 16, l192:5

Patented sept. 7,1926.

UNITEDy STATES.

q 1,599,360 PATENT OFFICE.

INGENUIN HEOHENBLEIKNER AND THOMAS C. OLIVER, OF CHARLOTTE' NORTH CAROLINA.

METHOD OIE' AND APPARATUS FOR SEPARATING PETROLEUM SL'UDGE.

Application led March 16, 1923. Serial No. 625,675.

This -invention relates to the recovering I of the components `of petroleum sludge obA tained in the refining' of oil, and more particularly to a method of and apparatus for effecting the separation of the petroleum sludge into its hydrocarbon and acid constituents; and has special reference to the provision of an apparatus in which the petroleum sludge may be efficiently treated at relatively high temperatures and pressures.

In the refining ofpetroleum, vthe crude oil or its fractional distillates is subjected to the action of sulphuric acid, the latter beingI used to react with the heavy hydrocarbons and other undesirable elements present in the crude oil; and as a result Vof this treatment there remains a sludge or acid tar which contains oil and other hydrocarbons combined with a dilutedl sulphuric acid. To recover the hydrocarbons and reclaim the acid, the sludge is treated to effect a separation of its hydrocarbon and acid components; and to effect this separation it has been proposed to mix the sludge with water and subject the mixture to heat at relatively high temperatures and pressures, this treatment resulting in the reclaiming of the oilconstituent and the restoring ,of the acid to a condition which permits of purification and concentration with ease.

In'carrying out the steps of thisseparation process, the sludge and water mixture is introduced into a closed vessel and is heated by applioation'of external heat to the, vessel, the mixture being subjected to heat 4at relatively high temperatures and pressures. In

the werking of the process a number of ob` jections and difficulties have been met with which have prevented in a large measure the successful adoption of the process on a commercial scale. It has been found, for example, that th vessels in which the sludge is treated are relatively short-lived, the vessels being attacked mechanically and chemically at the high temperatures and pressures employed. Where for example lead lined steel shell autoclaves have been used, we have discovered that the lead lining will flow, buckle and separate from the shell at the temperatures used, and vthat the lining will moreover be chemically attackedby 'the sulphuric acid component at the high temperatures, this resulting in not only shortening the life of the relatively expensive vessels, but in frequentbreakdowns and the consequent stopping 4of plant operation with the undesirable curtailing of the plant output incident thereto. To obviate these diiiiculties and to provide an apparatus which is contructed to successfully resist or withstand the destructive actions of the acid and heat A the vessels employed so constructed as to withstand'mechanical and chemical attack; and the still further provision of a method and apparatus for separating petroleum sludge or acid tar whichmay be practiced and operated 4with great economy, convenience and 'eiiiciencv To the accomplishment of thel foregoing and such other objects as will hereinafter appear, our invention consists lin the elements and their relation one'to vthe other, as hereinafter particularly described and soughtto be defined in the claims; reference being had to the 'accompanying drawings forming a part thereof, and in which Fig. l is an elevational view in cross-section of a vessel constructed in Vaccordance with the principles of our invention and employed in a continuous separation process,

Fig. 2 is a view taken in cross-section on the line 2-2, Fig. 1, and

Fig. 3 is an elevational view in cross-sec-A tion of a modified form of our invention employed in an intermittent or cyclic separation process.

- In practicing` the steps of the separation process in our invention, the petroleum sludge obtained as a product of the refining of petroleum oils ismixed with water and the mixture is subjected to the action of heat` at a relatively high temperature and by injecting steam into a body of the sludge mixture contained in a vessel, and by digesting the said sludge mixture with the steam at a temperature of aboutl 360 F. under pressure. this being preferably carried out apressure of about 6 atmospheres for a period of time ranging from 1 to 3 hours dependin upon the character or type of sludge eing treated, this treatment resulting in the separation of the sludge into its hydrocarbon and sulphuric acid components.

As heretofore stated, inthe Working of this processl the vessel in which the sludge isl heated is readily attacked by the heatL and the heated acid component, and the utilization of lead lined vessels has been found unsuccessful in practice, since the lead lining does not mechanically withstand thc heat and other reactions taking place in the vessel, and does not chemically resist the action of the hot acid component, with the result that the vessels are too short-lived for general commercial adoption. After extensive experimentation, We have empirically found that if the lead-lined vessel is provided With a second refractory lining such vas an acid-proof masonry lining so co-ordinated With the lead lining as to mechanically support the same and obviate the buckling and separation of the same from the vessel, and as to prevent chemical attack of the lead lining by the hot sulphuric acid, that the destructive tendencies of the reactions taking place may be substantially eliminated.

Referring now to Figs. 1 and 2 of the drawings, .We show a vessel generally designatedl as A built in accordance with our invention and used in the practice of our` continuous method of separating sludge described and claimed in. our copending application Ser. No. 626,272 filed March 20. 1923,v the said vessel A comprising preferably a cylindrical-shaped steel shell 10l vertically mounted upon a concrete foundation f, the said shell being provided With an intermediate vlining 11 made of lead and an 'inner masonry lining 12 which preferably comprises an acid-proof brick structure superposed on the lead lining 11 and functioning to mechanically support the same as well as to substantially prevent the sludge body 13 under treatment from reaching and attacking the same.

As described in our copending application above referred to, in the practice of the process a body of sludge mixture 13 is rst introduced into the vessel Aand'thereisubjected tothe action of steam injected into-- the vessel, 'the sludgev being heated to a teml perature preferably at about 360 F. under a pressure about 6 atmospheres for a period of from l to.3 hours, after which separate streams of sludge and steam are continuously and simultaneously injected into the vessel to effect a chemical separation of the vslud'geythe chemically separated components being continuously discharged from the vessel in quantities equal to the sludge mixture introduced therein. To accomplish VVfurther provided with a second inlet. duct 17' communicating With a steam supply line 18,-a' valve 19 being provided in this line for controlling the How of steam into the vessel. If desired, check valves 2() and 21 may be provided in the sludge and steam lines 15 and 18 respectively. In operation the sludge and steam streams are injected into the sludge body 13 at a predetermined rate so as to permit the sludge to be subjected to the heattreatment for a predetermined period, such as from about 1 to 3 hours, the treated sludge gradually rising to the top of the vessel by displacement for continuous discharge from the vessel for further treatment. j

For effecting a continuous discharge of the treated sludge, there is preferably provided adjacent the top of. the vessel A an overflow duct 22 controlled by a valve 23, the said duct communicating With a feed line 24 leading to other vessels (not shown), into which the chemically separated but mechanically intermixed sludge components are fed forobtaining a mechanical separation.

The vessel A may be provided with the pressure safety .valve 25 connected to the top 26 of the vessel and leading into the drain pipe 27. For reading the temperature conditions in the vessel, the usual pyrometer p may be employed.

Referring now to the modification shown in Fig. 3 of the drawings, the vessel B also com rises a verticall arranged cvlindricall ployed in a cyclic orintermittent process.

vIn the intermittent process the vessel B is ,first charged with a mixture 13 of sludge and Water. after which steam is injected into the sludge, heating the same to the desired temperature and pressure, the digesting With steam being carried on for a period ranging from about 1 to 3-l1ours, the. Eastern' sludges being capable of being treated for the lesser period, and the Western sludges for the greater period. After this treatment the contents of the vessel are allovvedv to settle, the sulphuric acid component gravitating to the bottom and the hydrocarbon constituent rising to the top, the thus physically separatedl components being then Withdrawn from lthe vessel prior to relling the same with anew charge. To accomplish these functions there is preferably provided a single duct 28 through Which the steam,

' a steam line'31 controlled byvalve 32, the

valves being operated to effect the desiredresults. For discharging the separated contents of the vessel-'there4 is provided -a-dis charge line 33 controlled by a valve 34,-the

-said line leading to acid and oil storage tanks (not shown). Thev duct 28 may if desired also be controlled by fa common valve 35. Also if desired the vessel B may be providedwith a safetyline similar to that heretofore` described, comprising a safety valve 25" connected to the top 26 of the vesselv and leading to a drainage pipe 27. vAlso the vessel B may be provided with the usual pyrometer p. l

While We have `shownour invention in the preferred forms, it will be obvious that many' changes and modifications rmay be made in the v'structure thereof, without departing from the spirit of the invention, deined in the following claimsa We claim:- v1. The method of separating petroleum sludge into its hydrocarbon and acid vconstituents which" comprises subjecting a mixture of petroleum sludge and water to the action of an internal-heat treatment at a high temperature and at al pressure greater than atmospheric in 'a closed pressure container having an exterior acid-proof lining and anv interior refractory facing for. the lining.

2.v The method of separating petroleum sludge into its hydrocarbon and acid constituents which comprises subjecting a mix-l ture of petroleum vsludgeand water-to the action of an internal heat treatment at a temperature of about '360 F. and a presv sure of about 6 atmospheres in a closed pressure 'container havingv an exterior acidproof lining and aninterior refractory masonry facing for the lining. 3. The method vofseparatmg petroleum.- sludge' intoits hydrocarbon .and acid constituents which comprises subjectnga'mixture of petroleum sludge and water in a ves sel having an exterior lead lining and an interior superposed masonry lining tothe ac tion of separated 4streams of steam and, sludge injected into the mixture to effect a reaction at a high temperature and, under a high pressure.

4. The method 'of separating petroleum sludge into its hydrocarbon ,andl acld constituents which comprises sub "ecti-ng a mixture of the petroleum sludge an A water in a vessel havlng an exterior lea-d lining and' an-*intef rior acid-proof brick lining to the'action of `an internal heat treatment at a' temperature 4 lof -about'360 F. and atmospheres. 4 5. An apparatus for use in treating petroa pressure of about 6 leum sludge at high temperatures and at pressures greater than atmospheric to effectl leum sludge at temperatures of about 360 F. and at pressures of about 6 atmospheres' to eiiect' a separation of the sludgeV into sludge oil and sludge acid, comprising a; pressure separator. consisting ofu-a'steel shell having an intermediate lead lining vand an' inner masonrylining adapted to withstand the action of the heat and the acid at the said temperatures andfpressures.

7 L An apparatus'foruse in treating petro leum sludge at temperatures of 'about 360-A F'. and at pressures of about 6 atmospheres to effect a separation of -the'fsludge'into sludge oiland sludge acid, comprising an autoclave-having an lntermedl'ate 'lea-d linl ing and A an inner supporting acid-proof brick lining adapted towithstand the action of the heat and the acid at the said temperatures and pressures.

' 8. An' apparatus for treating petroleum sludge at'temper'aturesfof about 360 F. andat pressures 4of 'about 6 atmospheres to effect a separationv of 1the sludge into sludge oil and sludge acid, comprising a vessel hav`n ing lan intermediatel lead lining and an inner masonry lining and separate inlet means for injecting simultaneously separate streams of steam4 andS sludge -into the vessel.

-' Signed by the saidl INenNmN HECHN BLE'IKNER', jat -Ohar'lotteyin the county' of Mecklenburg, and Stateof North Carolina, this1l2th day of-Marcli, A. D., 1923. j f

' IN GENUIN. HECHENBLEIKNER, j

Signed by the said 4THOMASl O. OLIVER at New York, in the county vof New York 'and State of New THOMAS C. OLIVER.

York-this 15th day of March,l 

